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"EDIBIr,» FILMS INCLUDING A,SkARTAME ~I~ Iv~THODS OJF MAY~TNG
~9!
~~A L .
13ACKGROUI~A Op' THE INVENTION
The present invention generally relates to edible film compositions. More
specifically, the present invention relates to edible films with inczeased
stability_
Aspartame has been used as am artificial, low calorie sweetener in numerous
food, cosmetic, a»d pharmaceutical cvznpositions. Aspartame is a very
attxaetive
sweetener due to xt$ intensity and because very Iow levels can be used tv
achieve a
high swee~ess perception by the consumer. It is noted for its clean, sweet
taste that
resembles sucrose. Aspartame has recently become a desirable sweetener to
employ iGn
edible film products.
Edible I'xlm groducts are designed to adhexe to azxd rapidly dissolve in the
mouth of the consumer. Edible films cant provide Ilavor ar~dlor oral care
agents, e.g.,
breath freshening to the consumer. Such films typically include a :film former
and
flavor or other iz~gredierct. See, for example, U.S. Patent No. 5,948,430 and
U.S.
Applicatioia publication No. US2001/Oa22964 AI.
Edible f [~, pxoducts are usually provided to the consumer in sta-ip form. The
strips are sized so that they can be placed o~n the tone of a consuiz~er. rn
this regard.,
the edible film strips typically have a size of a postage Stamp yr slightly
Iargez. These
strips pzeferably hava a supple texture and are non-self adhering.
Ono type of edible film product is distributed by Pfizer Consumer klealtheare
under the name ListerineG~ PocketPaksTM. The 1?;hzer edible film product is
packaged
in a plastic container that includes a top that can open along a hir~gc. A
stack of strips
are located in an interior of the paelcage one on lop of aztother. The package
is
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s
desig~zed so that the cansurxter can open tlae container azxd remove ozte
strip from the
stack with his or her fAngeT.
Edible fzim products aze also disclosed izt Assignee's co-pending U.S. parent
application "Rolled Edible Thin Film Products and IV~ethods of Making Same,"
Fled
on August 27, 2002, bearing x.1.5. Serial No. 101228,742.
Attempting to ixtcorporate aspartame in an edible film results in a less than
satisfactory product. The aspartame cant become unstable> yielding an
xrrferior, Iess
flavorful product. The ~ instability of aspartame is primarily due to tine
nature of
asparta~cze itself; its erystaIlirte structure and configuration. Aspartame
has historically
exlxibited difficulty in rs~aintaining its strucrure in complex, heterogeneous
environments. In pazticular> aspartame has two major disadvantages. 1~izst>
aspartame
becomes unstable under acidic conditions, and extaibits rapid degradation
wherx
exposed to elevated tezztpEratures. Secozxdly, the peptide nature of
aspartazrze makes it
susceptible to hydzalysis; this featufe also causes other reactions and
microbial
degradation.
Aspartame has previously dernoustrated instability izt other products, such as
chewing gums. Sugarless chervxztg gums often cozttain flavors aztd hygroscopic
compoztents that arc usually saturated with aldel~ydes that contribute to the
instability
of aspartame. The compozxents of a chewing guzza matrix generally yield a
product
having a pkZ of about ~.5. At this p~f, aspartame beeome;s unstable.
Similazly, the production of edible films also provide a complex rnatrxx of
ingredients and processing parameters that aid in rendering aspartame
unstable.
Therefore, there is a need far an edible frlmi product including aspaz~tame
that.is stable.
SUMMARY OF THE IN~V~E1V'~'ZON
The present irtvetation provides an edible ,filrxx pz'oduct with increased
aspartame
stability due to the incorporation of acid into the film far~ulation during
processing.
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1.t has been surprisingly discovered that by incorporati>3g . aczds into the
film
coating syrup dt~ning processing and maintaining a pH range o~F about 4.5 to
about 6,0,
tl~e aspartame will not denature in the final film carnpositiota, despite the
high
processing temperatures to which the film is exposed. !,
In accordance with the present xz~.vention, a variety of methods of foizning a
thin edible flm can be used. Ozte rzrethvd includes the st4~ps of. adding
filrn_forming
materials togethez- with water and agitating sarrae until tlae powder is
preferably
hydrated and few lumps are present. To this mixture, plasticizers, softening
agents,
colors, sweeteners, cooling agents, flavors and active ingredients can be
blended
together to form a homogeneous solution.
It should be ranted that err acid may be added at anytime before aspartame is
included into the mixture. Itr a pzefexxed embodiment, the acid is
incorporated aver
water has been added to the film forming materials to ztaal~e the coating
syrup. In an
embodiment of the process, a coatinb syrup with acid is then fed into a
hopper, and
spread onto a maving slebstrate through a drying tmuael in which it is exposed
to high
processing temperatures a~.~d exits the dzying system as a dried, edible
fitF.n. Upon
exiting the drying system, the filrrx may be rolled, cut, stamped, etched,
etc., to yield
the desired film form.
Irl an eznbodimeat of the present invention, at least one food grade acid is
added to the coatxzrg syzup.
In an embodiment, the acid is added to the coating syrup before water is
added.
1n an embvdirnent, the acid is added to the coatxz~g sy~p after water is
added.
In an embodiment, the acid is added to mixing lank before: other ingredients
are
added.
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In an embodiment of the present invention, the acid is chosen froze the group
consisting of phosphoric aczd; citric acid; make acid, acetic, adipxe,
benzoic, butyric,
formic, furnaric, hexanoic, lactic, propavnic, succinic, tartaric, carbonic,
attd sulforic.
In still another embodiment of the pz~esent invention, tl~e acid is
encapsulated.
In an errzbodiment, the acid is spray dxied.
In an ernbodizrzent, the pH of the coating syrup is between 4.7 and 5.~
In an embodiment, the pH oFthe coat~g syrup is between 4_5 and 6Ø
In an embodiment of the present invention, the acid maintains the stability of
the aspartame in the edible film con3positiozt during processing.
rn arr embodisner~t, the edible film compositiozt comprises at least one
polysaccharide.
In anoEhcr cmbodirn~ez~t, the edible film composition comprises at least one
filrta-forming agent drat is a water-soluble non-starch polysaccharide.
In an embodiment of the present invention, the film-forming ageztts include a
polysaccharide and a softener.
In an ernbodim~ent of the prcsezrt invention, the polysaccharide is pullulan.
lrt another embodiment of the present invention, the hltn product is a vehicle
for delivering active agents to a consumer.
In a fiuthe~r eznbodisnent of the present invention, a method for preparing a
rolled ~lrn is provided cornprisiag the steps of forming a rnixture of at
least one film
forming or coatixtg syrup material in powder form with a food grade acid and
water;
agitating the mixture preferably unizl the powder is txxostly hydrated and few
lumps
remain; adding to the mixture at least one ingredient selected from the group
Go~5I5tlIig of-. plasticizers, softening agents, colors, sweeteners, cooling
agetxts, flavors
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and active ingredients; blending the mixture to obtain a homagerteous
solution;
spreading the solution onto a moving substrate; drying the solution an the
substrate to
create a flexible ftlm.; a~,d winding the film onto a take-up roll- .
In an embodiment, a method for preparing a rolled film is pifovided comprising
forming a mixture of at least one .film-fvztning material in powder fornn and
water,
agitating the mixture until the powder is mostly hydrated and few lumps
remain,
adding to tlxe mixture at least one ingredient selected from plastieizws,
solfiening
agents, acids, colors, sweeteners, cooling agents, flavors and active
ingredielat$, then
adding aspartame, blending the mixture to obtain a homogeneous solution,
spreading
the solulzon vzztv a moving substrate, drying the solution on tk~e substrate
to create a
flexible film and winding the film onto a tape-up roll.
It is an advantage of the present inverttior~ to pzovide improved edible f
lms.
Another advantage of the present aravention is to provide a him corrtpositiott
including an acid that maintains the stability of aspartame during pzocessing.
Moreover, an advantage of the preseztt invention is to provide an improved
method ofmanufacturxzrg edible film products.
Still, an advantage of the present invention is to provide tua, edible film
product
including aspartame.
Another advazttage of the pzesezit izzventzort is to enhance the flavor of the
edible film_
Additionally, an advantage of the present invention is to provide methods for
stabilizing aspartame.
Furthermore, an advantage of the present iztvez~txor~ is that iv can be
:implemented by making relatively xniz~or modifications to an Otherwise
Conventional
process.
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Additional features and advantages of the present inventiozl are d~se~bed in.
and will be apparent in, the detailed desc~ption of the presently preferred
embodiments.
DETAILEI? ;DIrSCRIPTION OF THIS INVEl~'TION
'flxe present xzlventioa provides stable edible txlzn formulataor~so
containing
aspartame, through the: addition of acid to the film composition. Moreover,
the present
invention provides methods for manufacturing edible films eoataining
aspartame.
It has been surprisingly found to be advantageous during thin film processing
tv add acid to the film formulation. Pursuant to the present inventioxi,
aspartame
containing stable, flavoz~ul edible thin films can be formed by a variety of
difFei-ent
processes.
One such process xs as follows: (I) as adueous solution is formEd by blending
film-forrzzizlg materials to$othc~r with water and acid arid are agitated
until the
powdered materials are prefezably mostly hydrated and few lumps are present;
(2) to
ttus mixture, plastieizers, softening ageTlts, colors, sweeteners, cooling
agents, and
active ingredients are blended together to form a horxaogeneous solution; and
(3) this
solution is then cast auto a sutable carrier, and dried to fon~n a film. It
should be noted
that no particular order is placed on inevrporadclg the ingredients into tIze
mixture;
howwer, xt,is importarxt that the acid is included izt the solution before the
aspartame is
added. Tt should also be noted that a wide variety of film formulations or
coating
5yriip5 Carl be used.
As part of the process, preferably, a carrier is used to produce edible fihns.
T~xe
cannier material should be irctperr~cieable to the ;elm coating, allowing the
film coating to
disperse evenly oztto the carrier and allowing for the ease of removal of the
film from
the carrier. hxamples of suitable carriers include plastic or polyester films,
polypropylexte, polycarbonate, nva-siticonizcd polyethylene terephthalate
Film, .non-
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siliconized Kraft paper, polyethylene irtap~eegnated Kraft paper, metal belts,
voltage yr
corona treated belts, drum dryers, and polytetxaflurve2hylene-impregnated
glass fabric.
A particularly preferred method of casting the fllr'ta on the carrier is
tluough a
slot die extrusion- By use of mu2tiple .extrudErs and specially constructed
dies, it is
possible to add nnultiple color stripes to the p~oduCt. It is also possible tv
oscillate the
dze head tv produce wavy Lines on ttxe product. The resulting films eau be
laminated to
produce various visual ~ffeets.
The casting of the solution onto a suitable carrier material catr be performed
using any conventional coating technique. Examples of coating teclrniques
include
spraying, dipping, comma coatefis, l~nife over plate, roll aver roll, reverse
roll, slot die
extrusion, and various extrusion techniques. Fihxr thiclmess can be controlled
by
adjusting the gap on the coating head, or by applying the desired amount of
the
solution onto the substratelcarrier. No particular liruitation is placed an
the thiclrness
of the film layer. The thickness of the hlm may vary, or a mufti-layered film
product
may be processed, depending o~z the desired speed of dissolution o;f the
edible Fim
while in the oral cavity.
After coating, the film passes through a dryer for moisture reduction. Drying
is
carried out through a variety vl"different mesas, such as high velocity
turbulent hot air,
conduction from steam located slide bed, direct heating or casting o~ film
onto a heated
drum or belt, hot or cold six xznpingErnent, infrared heating, oz~ any other
suitable
drying eyupmertt tlxat dues not adversely affect the components of the film.
Once the film exits the drying system, the dried film is either taken-up along
with its substrate or peeled i~-om the carrier to form a wide roll. As the
film exits the
drying system, it can be exposed tv a number of different types of treatments.
If
desired, the film may be sprxztlsled with sugar, starch, flavor, color, color
enhancers
such as glitter, acids, bioadhesives, actives and texturizexs such as candy
sprinkles to
make specialty edible ftlrz~ products that may be desirable to younger
consumers.
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After the palm has bees dried arad treated as desired, it may be cut, stamped,
etched, punched, etc" into its final chosen sate and form. For example, the
edible filir~
can be a rolled edible filrt~_ Rolled edible films and methods of making the
same are
disclosed in U.S. Patent Application Serial t~tv. It?/228,742, entitled
"Rolled Edible
Thin Film Products and Methods of Making the Sajne," filed on August 27,2002,
the
disclosure which is incorporated herein by reference.
The formulations of the present inventiozz may be used to generate "specialty"
films that can be produced at various poizzts during the f~lzn making process.
For
example, those concepts which appeal to younger consumers. Types of specialty
filnrt
products include, but are not limited to films that are mufti-flavoring, mufti-
layering,
mufti-coloring, mult~i-shapes or foruzs, texturizing, larninatizrg, printing,
graphical
designs, "tongue-tattoos°°, oral sensations, varying dissoiuzion
pxofiles, bioadhesive
components, within the oral mueosa of a consumer; alone or in combinations
thez~evf.
The films of the present invention are also suitable for food applications
beyond direct
consumption.
Any suitable water-soluble, film-formex can be used to produce a rolled edible
thin film product, Suitable Flm-formers include, but are not limited tv, water-
soluble
non-starch polysaccharides such as modified eelIuloses, carboxymethylcellulose
(CMC), methylcellulose, hydroxypropylrrmthylcellulose (HI'MC), hydrolyzed
gums,
xanthan gum, guar gum, locust bean gum, tamarind, agar agar, carrageenau,
algins,
gum arabic, ghatti gurn, Karaya gum, Oragacanth gum, konjac, arabxzzvgalactan,
larch
arabinogalactan, beta-glucan, propylene glycol, pullulan, levan, elsinazi,
pullulan,
pectins, curdlan, chitosatz; native starches such as turn starch, waxy maize
starch, high-
amylose corn starch, potato, tapioca, rice and wheat starch; modified starches
sueb as
those that have been acid modified, bleached, oxidized, esterified,
ethcrified,
crossZxzxked, and treated enzymatically; starch hydz~olyzed products such as
maltodextrin: protein such as gelatin, casEin. salts of casein, whey, and
protein, derived
from soybeans; polymers such as polyvinyl pyrrolidone, methycrylate copolymer,
and
carboxyvinyl eopolyrz~ers alone or in any combinativzt. Iii an embodiment, the
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concentration of the film-forming agent constitutes between approximately 5%
to
about 60% by dry weights, or approximately 20% to abut 40% by dz7r weight of
the
hzral film composition. Further, it slavuld be noted that some ftIm forming
agents, such
as sodium alginate, will have an impact on the ~H of the edible film
composition.
i
Fiu ther, any suitable food-grade bulk filler can also be added to the elm.
This
cav reduce any "slimy" texture as well as provide structure io the film making
it more
palatable. In an erabodizactetit, the tiller can constitute approximately I%
to about 30%
by dry weigt3t of the film, ar approximately 5% to about 15% by dry weight of
the
fzlzzt, The filler can include microcrystalline cellulose, cellulose polymers,
such as
wood, magnesitun and calcium carbonate, ground limestone, silicates, such as
magnesium and alurnitzurn silicate, clay, talc, titanium dioxide, mono-calcium
phosphate, di-calcium phosphate, tri-calcium phosphate, other like bulk
fillers or
combinations thereof_
I,f it is desired to use reduced levels of f Inx forming agents; sofleneTs
coat also
be employed to ensure the flexibility of the film, thereby reducing
b~ttleraess. The
softetaers, which are also lrnowrz as plasticizers, may include tallow,
hydrogenated
tallow, hydrogenated and partially hydrogenated vegetable oils, cocoa butter,
sorbitol
and other polyols, glycerin, polyethylene gtycoJ, propylene glycol, invert
sugars, corn
syrup, lecitl~izt, hydrogenated lecithin, mono-, di- and trxglycerides,
acetylated
monoglycerides, fatty acids (c.g. stearic, palmitic, oleic, and linoleic
acids), arid
eornbinations thereof. In an embodiment, the so,~er~ex cdrr constitute 0% to
about 20%
by dry weight of the film, or approximately 2% to about 10% by dry weight of
the
Film.
Another means of controlliztg the brittlencss of the frlm as to maintain an
adequate moisture level in the hlm. Preferably, moisture levels should range
from
approximately 5°/q to about 20°/a or approximately 10°/V
to about l5% of brie final him
product.
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Pursuant to the preseztt invention, a variety of acids can be used to maintain
the
stability of the aspartame during processing or to enhance the flavor of the
filrtx. These
acids include, but, are not litnitcd to malic, fumarie, adipie, succinc,
citric, acetic,
lactic, pyruvic, butyric, foz~,ic; xsociiric, Iactocitric, shikirnic, quir>ic,
oxalic, glyceric,
citraznalie, glyeolic, ghxeuronic, galacturoinc, aspartic, benzoic,
lactarimic, cctostearic,
allantoic, pyroglutamic, hydrochloric, bexanoic, carbonic, sulfuric,
pyrrolidinonecarboxylic, and tartaric. Further, acids may be added to impact
the flavor
of the producf. For exanxple, malic acid is commonly associated with apples,
citric
acid with lemons, and tartaric acid with grapes_ However, mixtures of
different acids
may be used in combination to create a desired taste or flavor. Further,
t~tese acids
may be encapsulated to control their rate of zelease and interaction witkr the
other
components of the f lm matrix.
A variety of other suitable ingcdiezits cars be added to the edible flin of
the
present invention. For example, any suitable r~aedicament for oral clcansirng:
breath
Freshening or the like can be added to the .film formulation. The medicaments
can
xz~ctude, for example, pH control agents, tartar, caries control, whitenatxg
agerlts>
enzymes, breath freshening agents, anti,plaque/anti-gingivitis agezats, saliva
stimulating agents, pharmaceutical agents, nutxaceutical agents, vitamins,
mineral,
otlZer like rnedieaments or combinations thereof '
The: edible rIm fortn,ulations or coating syrups o,f the present invention can
also
include colorants or coloring agearts that can be used in any suitable amount
to produce
a desired color. Further, the rolled films of the present izzvention, if
desired, can
include colored stripes and/or other related desigrAS or shapes to produce
color
contrasts on the edible rolled film. Colaring agents can include, for example,
natural.
food colors and dyes suitable for food, drug, and cosmetic applications. The
colorants
are typically known as FD&C dyes and lakes-
1~ variety of flavoring ageztts can also be added to the edible frlms. - Any
suitable amount and type of artificial andfoz' ztatural flavoring agents can
be used izt any
sensorxally acceptable fashion. Far example, the flavor can constitute
approximately
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O.lp/° to about 20% by dry weight of the film, preferably
approxircaately 10% to about
15%. T'l~e flavoring agent can include, for example, essential oils, synthetic
favors or
r~zixtures including but not limited to ails derived from plants and fruits
such as citrus
oil, fruit essences, peppermint oil, : spearmint oil, other mint oils, clove
oils, oil of
wintergreen, anise and the like, favor oils with germ killing properties such
as
rraezzthol, eucalyptol, thyrriol, like flavotzng agents or combinations
thereof.
The flavor can be enhanced and distributed evenly throughout the product by
emulsi$catiozi, Any suitable amount and type of natural and/or synthetic food-
grade
emulsifier can be used. JFor example, the emulsifier can include lecithin,
:Coed-grade
non-ionic emulsifiers, such as fatty acids (C,o C,g), mono and diacyl
glyeerides, ox bile
extract, polyglycervl esters, polyethylene sorbitan esters, propylene glycol,
sorbitan
monopalmitate, sorbitan tristerate, other like emulsifiers or combinations
thereof:
The flavors can be emulsified by any suitable emulsircatioti process, such as
mechanical processing, vigorous stirring, intense pressure fluctuations that
occiu- in
turbulent flow such as homogenization, sotufieation, colloid milling acid the
like.
,~urth~r, flavors may also be encapsulated or spray dried onto the rolled
edible f'thn
product to enhazice flavor properties or to add texture tv the f lm
eomposidon.
Any siutable anriount of sweetening agents may also be employed for the
present xzzvention. Sugar sweeteners generally include saechuride-cvzttaining
cornpozients including but not li~ziting to, sucrose, dextrose, maltose,
dextrin, invert
sugar, ficuctvse, levulase, galactose, corn syrup solids, and the like, alone
or i~~ any
combination. Sugarless sweeteners z~zclude, but are not limited to, sugar
aIcohvls such
as sorbitol, manztitol, xylitol, isomalt, hydrogenated starch hydrolysates,
riialtitol, and
the Iike, alone vain any combination. ~Towever, the low weight of the Flan
picoducts of
tlae present invention generally tender these low intensity sweeteners
ineffective for
purposes of sweetening although t)xey nnay provide ft~netxvz~al benefits.
I-la~, intensity xrcificial sweeteners arc preferably used. alone or in
coriibination
with the above. Preferred sweeteners include, but are not li~riited to,
sueralose,
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aspartame, N-substituted AFM derivatives such as neota,ztte, salts of
acesulfame,
alitamc, saccharin and its salts, cyclamic acid and its salts, glycyrrhizin,
dihydrochalones, tlzaumatin, monellin, and the life, alone or in any
combination. In
order to provide enhanced yr d~:layed swaetncss, or to provide texture to the
roaled film
i
product, it may be desirable tip encapsulate the sweetener. Such teehniclues
as wet
granulation, wax granulation, spray drying, spray clxilling, fluid bed
coating,
cvacervation. and fiber extension may be used to achieve the de5xred
cl~araeteristies_
Combinations of sugar and/or sugarless sweeteners may be used in the film
pzoduct. Additionally, a softening agent may also provide additional sweetness
such
as with aqueous sugar or alditol solutions.
Cooling agents may also be employed in the present invention, cooling agents
include, but are not Iiznited tv> menthol, WS3, WS2~, Utzacool, monomenthyl
suceinate, alone or in any combination. Again, tk~ese cooling agents may be
encapsulated or spray dried onto the film to enhance a variety of oral
sensations.
Depending on the ingredierts being used to make the film pzvduct,
preservatives may also be employed to ensure the s~ety and quality of the
edzbae thin
film. Suitable preservatives include but are not Limited sorbic acid, svdaum,
benzoaee,
potassiur~z sorbate, methyl p-hydroxyber~zoate, sodium propionate, and propyl
p-
hydroxybenzoate alone or in any combination. In addition, suitable
antioxidants can
be used.
It should be appz~eciated Lbat any suitable type, number and arrar~gezrnent of
process procedures or sups (e:g. mixing, heating, dryiz~,g, cooling, addition
of
ingredients), process parameters (e.g: terrapezature, pressure, pFl, process
times) yr the
like can be utilized to practice the present invention.
~3y way of example and not limitation, exarcaples of tlxe present invention
will
now be given-
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Edible Filar Prepa>ratiou Method:
1:) Blending:
a
a) Powdered materials tsuch as film forming agents) are blended
together using a. ribbon blender or equivalent
b) Flavors or flavor components/cnhancers are blended together
using mecha~ica,1 agitation or equivalent.
2) Mixing:
a) 'fhe mixing tank is turned on and set at desired temperature.
b) To the mixilng Lank the blended powdered materials are added.
c) Water is added to the mixing lank, and begin agitation of the
mixing uank.
d) When alI water has been added, the desired acid is added.
e) Once all bleztded powders and acid have been added to the
mixing tarok, sweeteners, flaVOrs, cvlvxs, etc. are added as the temperature
rises. The
blend is maintained ai an even temperature, about 105 to about 115°F.
Tire conditions
of the mixing room are maitatained at about 70 to about 80°F, 40 to
about 50% RH.
3) Drying:
a) Feed solutivzt into a hopper.
b) Upon entering the drying system; the film solution is coated
onto a moving substrate which passes under a coma bar roll to produce a dry
thiclrness
of about 48 to about 52 microns.
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c) ,A,djust the beater temperature to achieve ara exit film
terzagezatwe of about 215 to about 220°F. This should produce a Flm
havir~~ a
moisture of about 9 to about 11 %.
d) ( Drying room conditions are about 70 to about 80°F, 40 tv about
50% RH.
4) C~ltting/Slzaping
a) The film is removed from the substrate upon exiting the drying
system and taken up on a separate roll. Unee the rolled deed Flm cools and
sets, it is
unwound and cut into its desized final lfvrrn_
Through quality assurance testing, it was discovered that after the edible
films
ltad been processed, tlae loss of aspartame was in a range of about 20 to
about ~0% in
the dal product after processuig. Several tests were run, incorporating acid
into tfle
filu~ composition in order to decrease or stop the losses of aspartarrie in
the final film
pxoduct. ~'he formulas used and the results from the tests rtxn are as
follows:
Fi~zished Wei~Zt
rngredieut Cvutroi Coulparative Example
x
Alginate 32.0 x'7.0
Maltodex?rin J 7.0 17,p
Garrageenan 12.0 a 2.0
Cellulose 10.0 10.0
Glyce~"in 8.5 8.S
Aspartame 1.0 1.0
Citric Acid -- 0.15
.Flavor 8.0 8.0
~.w...
5J5485/Dh FriCT01_ 14
CA 02479058 2004-08-25
menthol 1.5 1.5
Water 10.0 9.85
2"otul 100.0 ' 100.0
r
Test 1:
A syrup holding test was conducted to dernonsrrate aspartame de~adation in
the holding tazdt before the solution was processed attd dried to forrrt the
final film
product. Syrup was made with and without citric acid and placed in an oven at
125 to
about 133°k'. Samples of syrup were taken at 0, 2lxr, Shr, 24hr, 4$hr,
and 76hr.
Aspareame levels were tested, and the results arc as follows:
Time of SamplingCo~atrol ~:a;arrrrple x
(hrs.) (/v Aspartame (lV Aspartame
Retalped) Retained)
T = 0 I00v/o 100%
T= 1 92.0% d 00.0%
T= 5 87.0% X8.0%
T= 24 G I .U% 92_O%
T= 48 44.0% 8I .0%
'f= 76 34.0/v 73/v
The data above demonstrates a significant retention of aspartame while in
acidic solution over time. The contzol sample experia~zced a GG% loss of
aspartame
over a 76 hour period of tine. In contrssC, ~x~unple 1 (contaitun ; citric
.acid)
experienced only a 27% loss of aspartame over tk~e given period of time.
515485/DI1 F'NC3'oi_ 1$
CA 02479058 2004-08-25
Test Z
Dried syrup (final Eim product), was also tested for aspartame levels in the
fxzushed pzoduct. .Kandom samples were taken off the dried film role in the
begizminb,
middle, aid end regions of the roll. Aspartame levEls were determined froxu
each
region, and results ,are as follows:
Sampling region of Control Example 1
the roll (% Asparta~nac (% Aspartame
R,etx~iucd) Retained)
Begiruiing 76/Q 100%
Middle 66% 1 OU%
End 40% 98%
'flze data above demonstrates a significant loss of aspartame over tizne
(approxzzxaately 5 hours to complete the entire processing razz). The control
sample
experienced a 60% loss of aspartazzze over the five hour period, whereas
Example 1
(containing citric acid) onl~r Lost 2% aspartame.
Tlae following examples illustrate some ennbodiments of the invention. Qf
course, zrtay others are possible and arc easily Formulated by a skilled
technician once
ahe fuzadamez~taI concepts of the invention arc grasped.
5154851D1i F'I~tCT01_ 16
CA 02479058 2004-08-25
(% Finashed'OVt.)
Ingredieat ~, Ea.2 Ex.3 Ex.4 Eac.S Ex.6 Ex.7
Corn Starch 24.8 -- -- 30.0 -- --
F,lydroxyprvpylatrd- -- .- -- -- 47.35
Starch
Carrageenan . 14.0 I2.p 10.0 - 9.0 --
Glycerin 10.0 $.0 - 5_0 9.0 7.50
Gelatin - -- 12.0 S.0 -- 2.50
Microcrystalline 3.0 7.0 -- 5.0 8_0 --
Cellulose
Sodaumc~ A.lginxtc - 25.0 10.0 5_0 30.0 ?2,0
Maltodemrin -- X0.5 -- -- 18.0 -
Pallnlan 6.0 -- 39-0 - - --
Sorbitol 35_0 - -- 5.0 -- --
Liquid Sorbitol -- -- - I O-0 - --
tl,cesullamie ~ - -- -- -- -- 1.0
Sacralosr - 1.45 1.U 1.0 -- 1
_25
Aspartame I -50 -- 2.0 -- 2.0 --
WS-3 - I.55 - I _0 -- --
WS-23 -. -- 2.0 -_ __ -_
Menthol -- 6_0 1.0 -- 3.0 ' 1.0
Spearmint __ -. __ __ 6.0 __
Cherry Flavor 15.0 5.0 -- F2_0 - _
Ptppc~-nniatt~ _ __ __ __ 6.U __
)vwcalyptol - -- -- - -- 6.00
S15a8S1pi1 FriC't'O1_ I7
CA 02479058 2004-08-25
Methyl Salicylate - 4.$ IO_0 _ _ ._
Citric Acid __ 0.1 -- 5.0 I .0 _.
Adipic .Acid -- __ l ,p __ __ 1.00
~'l~osphvric 0-2 0.1 - -- _ __
Acid
Cvlor ~ 0.50 O.SO -- 0-SO 0.35 0.X0
Water 10.0 8.0 12.0 1S_S 7.65 10.0
Tertal 100.0 100.0 100.0 100-0 100.0 100.0
SISaBSIOI~ FNCTOi_
CA 02479058 2004-08-25
Ingredient Ea.8 Ea.9 I:a.lO' E~.11 Ea.l2 Fx.l3
I3yd: oxyethylated Starch-- ~i8.0 .- -_ _. __
PURt~-COTE~ >8790* 50.0 -_ _,. __ __ __
Enzyme Flydrotyzed Corn -- -- 22.0 -- - --
Stare6
Maltodextrin -- -- 5.0 28.0 -- --
Casein -- 2.9 - -- 3.S -
~'ullulnn _ __ ._ __
20.0 35.0
Polyvinyl Pyrollidane -- 11.0 -- -- 6_0 --
~
Hydroaypropylmcthylcetlotosc- -- -- -- 30.0 --
Xanthan Guut -- -- -- -- -- 6.0
Locust l3aan Cum -- -- -- -- -- 8.0
Glyerin -- -- -- 12.0 9.5 10,5
kolyctl~yteue Glyeot - -- -- -- 6.0 --
Propylene Glycol 1.50 -- i 0.0 -- G.0 --
Carrageenan - 11.0 - 10.0 -- 24.7
Sodium Alginate -- - -- i3.75 -- -.
Calcium Al~in~atr ~ 22.9 -- -- ~. -- -
SilfCa -- -- -- 5.0 -- -
Calcium Carbonate - -- 3.0 -- - --
~CCtjdt 4,0 - -- _.. - __
l~ccithi~z - 2-0 1-0 1.5 __ _
Saccharin - __ _- .. __
2.0
A,spartamc 0.25 -- - 1.0 1.5 _..
Sucralosc 1.25 -- -- -- -- --
s~sassrn~~ r~~To~_ 19
CA 02479058 2004-08-25
Neota~ue -- -- 0.50 -- ).S --
Encapsulated Acesuif-.~a~e -- -- 1.5 -- 1.0 --
K
15_0
Corn Syrup . _- ._ __ _
l
'. Guar Gam -- 2.0 -- -- -- --
Sorbitan Moaopalsr~itate -- -- -- -- 4.0 --
Ultracool - -- -- 1.2 -- 5.0
.
Citrie Acid - -- -- 1.5 -- --
Adipic Acid _. _- -_ 1.5 .- .-
JV~ethy! Salieylate -. ' __ .. -- _ 1.S
EucaIyptol -- 6.0 -- -- -.. 0.5
iI"Atymol -- _- 2.8 -_ _ 0.5
Encapsulated Peppermint -- -- -- -- 1 i.0 --
Mcrrtlaot -- -- 8_0 -- 4_0 I_5
Lert~oa Flavor 10,0 -- -- 8.0 -- --
Mixed Berry Flavor -- 5.0 -- 8.0 --
Fumaric ,A,cid 1.0 005 - 0.1 -- --
Tartaric Acid -- -- 0.1 U.1 -- 0.30
Citric Acid -- -- 0.1 0,1 I.0 --
Color 0.05 0-OS 0.50 0.25 -- 0.5
~Vntcr 9.05 12.0 10.5 8.0 15.0 4.0
'Total 100.0 100,0 100.0 100.0 100,0 100_0
'k PURE-COTE~ B'79fl g Corporation
is a produet of the (Gl'C),
Grain Processin located
is
Muscatine, Iowa. PITRE-CVTE~ ash-d7ried rch designed
B'79fl ruodilied spacitacally
is corn
a sta
fl
for applicotions 1'cyuiriag
very low viscosity.
515dR5ipli FNC-fUl_ ~o
CA 02479058 2004-08-25
Irag~r~edient Ex, Ea. Ea. h,~. fix. h~s.X8 ~x.~9 ELK.
13 1~ 15 lb 17 2
Ilydroxypropylccllulosc~S-0 -- , -- - -- -- 18.0 -
Waxy Maize Starch - -- -- -- - -- 15.0 --
Potstv Starch 2.0 -- 29.5 -- -- .- .. ..
JPuIfulan . 26-0 8.0 -- 55.0 .. .. -.
Microcrystalline Cetlalose- -- I O.U 6.5 -- 8.0 -- G.5
Sorbitaa Fatty Acid -- 1.0 -- -- -- 3.0 --
Ester
Matiodexiri><a - 19.0 - 2p,0 -- 28-0 -- I9-0
Carrage~nan -- 16.0 -- 10_0 -- 8_0 1.5 10.0
Gclatir~ 7.0 __ __ ._ Z.0 __ .. ._
PolyYinyl Alcoiiot 5.85 -- _. -_ _ _- _ _-
Sodium I'olyacryl:dte 5.0 -- - -- -- - ~ -- --
Csa~rb4xyrnethylccllulose5_0 -- -- -- -- -- -- -
Xantban Cu -- 3.0 -- -- -- -- - --
Karsya Gum 3.5 -- -- -- 6-U -- -
Glycerin _- __ G.0 -- 4.5 _. 6.0
'1'itaniam Dioxide . -- 2.0 __ ._ .. 2.S __
Sodium Al~inmc - -- -- 25.0 2.0 20.5 13.0 19.0
Sorbitol - -- 1.5 - -- 0.05 -- --
Encapsulated Aspartpme -- -- -- -- ~- -- 1.0 --
Suc=atone - -- -- -- -- 1.5 1.0 3.0
Corn Syrug _ _- 15.4 _- .- ... .. __
Soybean Oal - - I.0 - __ __ __ _
Lecitbin - -- -- I.5 0.5 0.50 - 1.5
515a8Slplf FNCTOI_ Z1
CA 02479058 2004-08-25
Dextrv5e __ _ Z.0 .- __ __ _. _
~ruciose - 9.5 _. __ $.0 .. _. ._
'WS-3 - 2.9 .. D -0 -- - 4.0 0.5
Clove Oil - -- 1,0 -- 4.5 - -. -_
tYlenthol 8.0 2.U -- 2_0 -- -- 1.0 O,S
Grape Flsvor - -- -- -- -- -- 12_0 5.0
Lemon Blavor - _ __ __ __ 5.0 _- __
Rose Oil __ Z.0 -- - .. __ I,p ._
Pepper - 2.0 -- -_ __ __ _- __
O~'~nge ~'tavor -- -- 3.0 -- -- 4.0 2_0 _.
Peppcra~int OiI .. - -- 9.0 5.0 2.0 -- --
Cardamom 8.0 2.0 .. __ _ 1.0 __ __
Crapeseed E:tract - -- -- 5.2 Z.S -- -- -
Tea Catecltixts - .. .. __ __ I.0 __ __
Yitattnia C ._ __ 3.0 -- 2_S __ 5.0 9_9
Vitamin .A,B,D,E Comglex. .. __ __ __ .. .. 5.0
Zinc Glucv~ate - - -- -- -- -- 5.0 1.0
Suecinic Acid -- 0.2 - -- -- 1.S -- 0.001
Ts~rtaric Acid 0.15 -- -- 1-0 -- -- -- 3-0
Eacapsutated Citric 0.3 Z,0 - -- 5.0 S.0 --
Acid
Ecttinacea - - 3.0 -- 2.5 1.0 -- --
~
CetyI Pyridinium Cltloside3.0 .. -- -- __ __ _ ._
Encapsulated Caffeine - 5.0 -- -- -. _. __ __
Sodium Bcnzonatc ..- -- 2_0 0.5 -- -- -_
315485/D/I f'NCTQt_
CA 02479058 2004-08-25
u.
)<iFiA - -- 0.5 -- 0,0s _. __
Color 0.5 0.1 O.G 0.30 0,5 0,80 0.1 0.1
WRter 7.0 10.0 17.0 10.0 11.5 7.6 ~:9 9.999
Total 100.0 100.0 , 300,0 100,0 100,0 100.0 100.0 100,0
s~saxsmn rNCn'o~_ ~3
CA 02479058 2004-08-25
It should be appreciated that various changes axtd mod~i~eations of the
presently
preferred etnbodxmer~ts described herein will be apparent to those skilled in
the art_
Such chang4s at~d modifications can be axxadE without departing from the
original spirit
and scope of the presezct invention without diminishing its intended
advantages. It is
therefore intended that such changes and modificarions be covered by the
apper~de~d
clairr~s_
s~sassrnr~ ~cTO~_
